CN-122011770-A - Flame-retardant charring agent and preparation method and application thereof
Abstract
The invention provides a flame-retardant char-forming agent, a preparation method and application thereof, and belongs to the technical field of flame-retardant materials. The invention adopts a modifier to carry out modification treatment on organic silicon resin, adopts a silane coupling agent to carry out surface treatment on ceramic powder, adopts an acetylating agent to carry out acetylating treatment on lignin, then dries the obtained modified organic silicon resin, carries out melting treatment, adds the obtained surface treated ceramic powder to carry out first banburying, and adds the obtained acetylating modified lignin, a biocompatible agent, magnesium oxide and aluminum oxide to carry out second banburying to obtain the flame-retardant carbonizing agent. The flame-retardant char-forming agent has good interfacial compatibility, compact and stable formed carbon layer, and excellent flame-retardant property and mechanical property of the prepared flame-retardant material.
Inventors
- CHEN JIANQING
Assignees
- 苏州百研阻燃材料有限公司
Dates
- Publication Date
- 20260512
- Application Date
- 20260309
Claims (10)
- 1. The preparation method of the flame-retardant char-forming agent is characterized by comprising the following preparation steps: mixing the organic silicon resin with a modifier, and carrying out modification treatment to obtain modified organic silicon resin; mixing the porcelain powder with a silane coupling agent, and performing surface treatment to obtain surface-treated porcelain powder; drying lignin, dispersing the lignin in a solvent, adding a catalyst and an acetylating reagent, and performing an acetylating reaction to obtain acetylating modified lignin; Drying the modified organic silicon resin, performing melting treatment, adding the surface treatment porcelain powder, performing first banburying, then adding the acetylated modified lignin, the biocompatible agent, the magnesium oxide and the aluminum oxide, and performing second banburying to obtain a flame-retardant char-forming agent; the modifier comprises gamma-aminopropyl triethoxy silane, gamma-glycidol ether oxypropyl trimethoxy silane or isocyanatopropyl methyl dimethoxy silane.
- 2. The method of preparation of claim 1, wherein the silicone resin comprises methyl phenyl silicone resin or methyl vinyl silicone resin; the mass of the modifier is 1% -5% of the mass of the organic silicon resin; the temperature of the modification treatment is 60-80 ℃ and the time is 2-4 h.
- 3. The method of producing according to claim 1, wherein the silane coupling agent comprises vinyltrimethoxysilane or vinyltriethoxysilane; the mass of the silane coupling agent is 0.5% -3% of the mass of the porcelain powder; The temperature of the surface treatment is 60-80 ℃ and the time is 1-3 hours; the average grain diameter of the surface treatment porcelain powder is 1-10 mu m.
- 4. The preparation method of claim 1, wherein the drying temperature is 60-80 ℃, and the solvent comprises glacial acetic acid, ethanol or 1, 4-dioxane; The catalyst comprises one or more of pyridine, triethylamine, sulfuric acid and p-toluenesulfonic acid, and the mass of the catalyst is 1% -5% of the mass of the lignin; The acetylation reagent comprises acetic anhydride, and the mass ratio of lignin to the acetylation reagent is 1:0.5-1; The temperature of the acetylation reaction is 70-85 ℃ and the time is 3-5 hours; the acetylation degree of the acetylation modified lignin is 20% -30%.
- 5. The preparation method according to claim 1, wherein the temperature of the drying is 80-90 ℃ and the time is 3-4 hours; The temperature of the melting treatment is 100-120 ℃ and the time is 10-25 min; The temperature of the first banburying is 100-120 ℃ and the time is 45-80 min; The biocompatible agent comprises maleic anhydride grafted polypropylene or maleic anhydride grafted polyethylene; the temperature of the second banburying is 100-120 ℃ and the time is 40-60 min.
- 6. The preparation method of claim 1, wherein the mass ratio of the modified silicone resin to the surface-treated porcelain powder is 10:6-8.
- 7. The preparation method of claim 1, wherein the mass ratio of the modified silicone resin to the acetylated modified lignin, the biocompatible agent, the magnesium oxide and the aluminum oxide is 10:1-2:0.5-1.5:3-5:3-5.
- 8. The flame retardant char-forming agent prepared by the preparation method according to any one of claims 1 to 7.
- 9. The application of the flame-retardant char-forming agent in flame-retardant materials, which is characterized in that the flame-retardant materials are prepared from the following components, by mass, 100 parts of thermoplastic polyolefin, 100-150 parts of inorganic flame retardant and 5-15 parts of char-forming agent; the char-forming agent is the flame retardant char-forming agent according to claim 8.
- 10. Use according to claim 9, wherein the thermoplastic polyolefin is polypropylene and the inorganic flame retardant comprises aluminium diethylphosphinate or aluminium hydroxide.
Description
Flame-retardant charring agent and preparation method and application thereof Technical Field The invention relates to the technical field of flame-retardant materials, in particular to a flame-retardant char-forming agent, a preparation method and application thereof. Background With the wide application of high polymer materials in the fields of construction, electronic and electric appliances, transportation and the like, the fireproof safety of the materials is increasingly important. As a key auxiliary agent for improving the fireproof performance of the high polymer material, the research, development and application of the flame retardant become important research directions in the field of material science. The intumescent flame retardant system can promote the surface of the polymer to form an intumescent carbon layer in the combustion process, effectively isolates heat and oxygen, has the environment-friendly characteristics of low smoke, low toxicity, no molten drop and the like, and becomes one of the main development directions of halogen-free flame retardant technology. The char former serves as the core component of the intumescent flame retardant system and its primary function is to provide a source of char during the combustion process to promote the formation of a dense char layer. However, the traditional char forming agent has poor compatibility with a polymer matrix, uneven dispersion is easy to occur in the processing process, the mechanical property of the material is influenced, the flame-retardant stability is reduced, the high-temperature thermal stability of part of the char forming agent is insufficient, a continuous and compact char layer is difficult to form in the initial stage of combustion, the separation efficiency is low, and the heat release and the smoke generation cannot be effectively inhibited. Disclosure of Invention The invention aims to provide a flame-retardant char-forming agent, a preparation method and application thereof, wherein the flame-retardant char-forming agent has good interfacial compatibility, a formed carbon layer is compact and stable, and the prepared flame-retardant material has excellent flame retardant property and mechanical property. In order to achieve the above object, the present invention provides the following technical solutions: the invention provides a preparation method of a flame-retardant char-forming agent, which comprises the following preparation steps: mixing the organic silicon resin with a modifier, and carrying out modification treatment to obtain modified organic silicon resin; mixing the porcelain powder with a silane coupling agent, and performing surface treatment to obtain surface-treated porcelain powder; drying lignin, dispersing the lignin in a solvent, adding a catalyst and an acetylating reagent, and performing an acetylating reaction to obtain acetylating modified lignin; Drying the modified organic silicon resin, performing melting treatment, adding the surface treatment porcelain powder, performing first banburying, then adding the acetylated modified lignin, the biocompatible agent, the magnesium oxide and the aluminum oxide, and performing second banburying to obtain a flame-retardant char-forming agent; the modifier comprises gamma-aminopropyl triethoxy silane, gamma-glycidol ether oxypropyl trimethoxy silane or isocyanatopropyl methyl dimethoxy silane. Preferably, the silicone resin comprises methyl phenyl silicone resin or methyl vinyl silicone resin; the mass of the modifier is 1% -5% of the mass of the organic silicon resin; the temperature of the modification treatment is 60-80 ℃ and the time is 2-4 h. Preferably, the silane coupling agent comprises vinyltrimethoxysilane or vinyltriethoxysilane; the mass of the silane coupling agent is 0.5% -3% of the mass of the porcelain powder; the temperature of the surface treatment is 60-80 ℃ and 1-3 hours; the average grain diameter of the surface treatment porcelain powder is 1-10 mu m. Preferably, the drying temperature is 60-80 ℃, and the solvent comprises glacial acetic acid, ethanol or 1, 4-dioxane; The catalyst comprises one or more of pyridine, triethylamine, sulfuric acid and p-toluenesulfonic acid, and the mass of the catalyst is 1% -5% of the mass of the lignin; The acetylation reagent comprises acetic anhydride, and the mass ratio of lignin to the acetylation reagent is 1:0.5-1; The temperature of the acetylation reaction is 70-85 ℃ and the time is 3-5 hours; the acetylation degree of the acetylation modified lignin is 20% -30%. Preferably, the temperature of the drying is 80-90 ℃ and the time is 3-4 hours; The temperature of the melting treatment is 100-120 ℃ and the time is 10-25 min; The temperature of the first banburying is 100-120 ℃ and the time is 45-80 min; The biocompatible agent comprises maleic anhydride grafted polypropylene or maleic anhydride grafted polyethylene; the temperature of the second banburying is 100-120 ℃ and the time is 40-60